#------------------------------------------------------------------------------ #$Date: 2021-07-22 05:42:51 +0300 (Thu, 22 Jul 2021) $ #$Revision: 267690 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/78/7707871.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7707871 loop_ _publ_author_name 'Chen, Sun' 'Oswald, Victoria Frances' 'Hill, Ethan A.' 'Ziller, Joseph W.' 'Borovik, Andrew' _publ_section_title ; Investigation of Iron--Ammine and Amido Complexes within a C3-Symmetrical Phosphinic Amido Tripodal Ligand ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01032H _journal_year 2021 _chemical_formula_sum 'C62 H85 Cl4 Fe K N7 O9 P3' _chemical_formula_weight 1402.03 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-01-02 deposited with the CCDC. 2021-07-20 downloaded from the CCDC. ; _cell_angle_alpha 101.9506(7) _cell_angle_beta 98.9294(7) _cell_angle_gamma 118.7866(7) _cell_formula_units_Z 2 _cell_length_a 14.6635(7) _cell_length_b 14.8610(7) _cell_length_c 18.8343(9) _cell_measurement_reflns_used 9861 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 28.74 _cell_measurement_theta_min 2.32 _cell_volume 3360.0(3) _computing_cell_refinement 'Bruker SAINT 8.34a, 2013' _computing_data_collection 'Bruker APEX2 2014.11-0, 2014' _computing_data_reduction 'Bruker SAINT 8.34a, 2013' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'Bruker SHELXTL 2014/4' _diffrn_ambient_temperature 133(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_unetI/netI 0.0216 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 39019 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.102 _diffrn_reflns_theta_min 1.157 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_T_max 0.8015 _exptl_absorpt_correction_T_min 0.7193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS 2014/5' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_meas ? _exptl_crystal_density_method not_measured _exptl_crystal_description prism _exptl_crystal_F_000 1472 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: dichloromethane, pentane' _exptl_crystal_size_max 0.393 _exptl_crystal_size_mid 0.391 _exptl_crystal_size_min 0.178 _refine_diff_density_max 0.912 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 804 _refine_ls_number_reflns 14722 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0365 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+3.1983P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.0943 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13000 _reflns_number_total 14722 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01032h2.cif _cod_data_source_block asb550 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_density_meas' value 'not_measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 3359.9(3) _cod_database_code 7707871 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.805 _shelx_estimated_absorpt_t_max 0.904 _exptl_absorpt_special_details ; Reflections not merged 40636 Corrected reflections written to file asb550s.hkl Estimated minimum and maximum transmission: 0.7193 0.8015 The ratio (0.8974) of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.1500 Lambda/2 correction factor = 0.00150 ; _shelx_res_file ; asb550.res created by SHELXL-2014/7 TITL asb550 in P-1 rem APEX2 2014.11-0, SAINT 8.34a, SADABS 2014/5, SHELXTL 2014/7 CELL 0.71073 14.66350 14.86100 18.83430 101.9506 98.9294 118.7866 ZERR 2.00 0.00070 0.00070 0.00090 0.0007 0.0007 0.0007 LATT 1 SFAC C H N O P Cl K Fe UNIT 124 170 14 18 6 8 2 2 L.S. 10 PLAN 10 SIZE 0.178 0.391 0.393 TEMP -140 HTAB N5 O1 HTAB N5 O2 HTAB N5 O3 FREE C62B Cl4A FREE C62 Cl4B FREE C62 C62B FMAP 2 SHEL 100 0.78 ACTA WGHT 0.043000 3.198300 FVAR 0.10390 FE1 8 0.724390 0.400688 0.129980 11.00000 0.01116 0.01105 = 0.01167 0.00317 0.00317 0.00567 P1 5 0.710705 0.188532 0.171345 11.00000 0.01275 0.01253 = 0.01697 0.00481 0.00287 0.00720 P2 5 0.962589 0.624294 0.162462 11.00000 0.01326 0.01274 = 0.01610 0.00217 0.00535 0.00531 P3 5 0.540209 0.446336 0.180007 11.00000 0.01364 0.01374 = 0.01612 0.00624 0.00574 0.00843 O1 4 0.777819 0.261128 0.251164 11.00000 0.01818 0.01893 = 0.01807 0.00488 0.00138 0.01031 O2 4 0.959495 0.667420 0.240490 11.00000 0.01919 0.01976 = 0.01861 -0.00026 0.00582 0.00691 O3 4 0.584953 0.450524 0.258530 11.00000 0.02051 0.02090 = 0.01728 0.00789 0.00705 0.01298 N1 3 0.661038 0.337427 0.004010 11.00000 0.01404 0.01194 = 0.01325 0.00308 0.00359 0.00652 N2 3 0.846718 0.528054 0.103245 11.00000 0.01359 0.01443 = 0.01432 0.00330 0.00480 0.00511 N3 3 0.713201 0.250146 0.109845 11.00000 0.01555 0.01242 = 0.01496 0.00346 0.00334 0.00734 N4 3 0.574645 0.391716 0.114822 11.00000 0.01376 0.01630 = 0.01467 0.00479 0.00338 0.00903 N5 3 0.790153 0.467812 0.251296 11.00000 0.01496 0.01765 = 0.01385 0.00423 0.00394 0.00580 H5A 2 0.805527 0.426315 0.268585 11.00000 0.05075 H5B 2 0.844096 0.529320 0.263011 11.00000 0.03469 H5C 2 0.744555 0.473867 0.266644 11.00000 0.02858 C1 1 0.719430 0.428669 -0.023766 11.00000 0.02300 0.01762 = 0.01461 0.00736 0.00614 0.01013 AFIX 23 H1A 2 0.686077 0.473004 -0.019905 11.00000 -1.20000 H1B 2 0.712893 0.400354 -0.077934 11.00000 -1.20000 AFIX 0 C2 1 0.839012 0.499158 0.022250 11.00000 0.01889 0.01547 = 0.01508 0.00452 0.00677 0.00678 AFIX 23 H2A 2 0.875876 0.459111 0.011697 11.00000 -1.20000 H2B 2 0.875161 0.565754 0.008061 11.00000 -1.20000 AFIX 0 C3 1 0.683769 0.252071 -0.021049 11.00000 0.01967 0.01773 = 0.01601 0.00224 0.00593 0.01125 AFIX 23 H3A 2 0.761239 0.285714 -0.019725 11.00000 -1.20000 H3B 2 0.638337 0.206556 -0.074133 11.00000 -1.20000 AFIX 0 C4 1 0.659862 0.181254 0.029650 11.00000 0.01837 0.01305 = 0.01814 0.00265 0.00383 0.00848 AFIX 23 H4A 2 0.580180 0.135946 0.020518 11.00000 -1.20000 H4B 2 0.687111 0.132331 0.017460 11.00000 -1.20000 AFIX 0 C5 1 0.543847 0.294683 -0.016588 11.00000 0.01454 0.01929 = 0.01624 0.00212 0.00074 0.00853 AFIX 23 H5D 2 0.504387 0.220989 -0.012396 11.00000 -1.20000 H5E 2 0.517736 0.289090 -0.069984 11.00000 -1.20000 AFIX 0 C6 1 0.519799 0.368464 0.035363 11.00000 0.01613 0.02092 = 0.01606 0.00457 0.00192 0.01138 AFIX 23 H6A 2 0.545957 0.437107 0.023592 11.00000 -1.20000 H6B 2 0.440198 0.332569 0.026968 11.00000 -1.20000 AFIX 0 C7 1 1.021268 0.735765 0.124113 11.00000 0.01172 0.01396 = 0.02228 0.00382 0.00382 0.00508 C8 1 1.015694 0.826452 0.154642 11.00000 0.01568 0.01744 = 0.02494 0.00163 0.00228 0.00816 AFIX 43 H8 2 0.986696 0.830207 0.196132 11.00000 -1.20000 AFIX 0 C9 1 1.052352 0.911136 0.124614 11.00000 0.01870 0.01582 = 0.03867 0.00479 -0.00140 0.00968 AFIX 43 H9 2 1.049635 0.973108 0.146453 11.00000 -1.20000 AFIX 0 C10 1 1.092669 0.906094 0.063377 11.00000 0.01499 0.02182 = 0.03723 0.01519 0.00067 0.00559 AFIX 43 H10 2 1.116564 0.963893 0.042732 11.00000 -1.20000 AFIX 0 C11 1 1.098233 0.816398 0.032010 11.00000 0.01452 0.02719 = 0.02814 0.01196 0.00681 0.00741 AFIX 43 H11 2 1.125522 0.812405 -0.010349 11.00000 -1.20000 AFIX 0 C12 1 1.063690 0.732319 0.062835 11.00000 0.01476 0.01821 = 0.02796 0.00612 0.00800 0.00776 AFIX 43 H12 2 1.069042 0.671747 0.041906 11.00000 -1.20000 AFIX 0 C13 1 1.057302 0.577885 0.169496 11.00000 0.01763 0.01966 = 0.01490 0.00562 0.00620 0.00990 C14 1 1.169476 0.649796 0.202598 11.00000 0.01965 0.02031 = 0.02446 0.00183 0.00545 0.00832 AFIX 43 H14 2 1.199167 0.725823 0.216845 11.00000 -1.20000 AFIX 0 C15 1 1.238040 0.611433 0.214908 11.00000 0.01680 0.03253 = 0.02407 0.00348 0.00345 0.01167 AFIX 43 H15 2 1.314197 0.661258 0.237619 11.00000 -1.20000 AFIX 0 C16 1 1.195987 0.500852 0.194243 11.00000 0.02803 0.03624 = 0.02348 0.01132 0.00970 0.02303 AFIX 43 H16 2 1.243045 0.474801 0.203162 11.00000 -1.20000 AFIX 0 C17 1 1.085009 0.428329 0.160508 11.00000 0.02831 0.02382 = 0.03394 0.01122 0.00900 0.01620 AFIX 43 H17 2 1.055988 0.352403 0.145802 11.00000 -1.20000 AFIX 0 C18 1 1.016118 0.466504 0.148161 11.00000 0.01865 0.01869 = 0.02574 0.00647 0.00524 0.00833 AFIX 43 H18 2 0.940125 0.416298 0.124943 11.00000 -1.20000 AFIX 0 C19 1 0.755387 0.095618 0.140690 11.00000 0.01659 0.01506 = 0.02169 0.00927 0.00761 0.00989 C20 1 0.861298 0.126885 0.177775 11.00000 0.01795 0.01986 = 0.02411 0.00793 0.00505 0.01045 AFIX 43 H20 2 0.904544 0.190871 0.220744 11.00000 -1.20000 AFIX 0 C21 1 0.903859 0.064803 0.152124 11.00000 0.01650 0.02725 = 0.03284 0.01159 0.00655 0.01398 AFIX 43 H21 2 0.975868 0.086451 0.177834 11.00000 -1.20000 AFIX 0 C22 1 0.841632 -0.028598 0.089161 11.00000 0.02431 0.02365 = 0.03333 0.01502 0.01617 0.01772 AFIX 43 H22 2 0.871393 -0.070099 0.071333 11.00000 -1.20000 AFIX 0 C23 1 0.736031 -0.061078 0.052422 11.00000 0.02264 0.01520 = 0.02725 0.00861 0.01023 0.01035 AFIX 43 H23 2 0.693126 -0.125127 0.009476 11.00000 -1.20000 AFIX 0 C24 1 0.692897 0.000005 0.078381 11.00000 0.01608 0.01559 = 0.02672 0.00911 0.00648 0.00864 AFIX 43 H24 2 0.619971 -0.023445 0.053496 11.00000 -1.20000 AFIX 0 C25 1 0.570036 0.100457 0.169868 11.00000 0.01444 0.01461 = 0.01496 0.00298 0.00390 0.00646 C26 1 0.539885 0.012857 0.197400 11.00000 0.01961 0.01911 = 0.01594 0.00526 0.00399 0.01126 AFIX 43 H26 2 0.591683 -0.005545 0.213049 11.00000 -1.20000 AFIX 0 C27 1 0.434570 -0.047603 0.202059 11.00000 0.02274 0.01715 = 0.01563 0.00561 0.00645 0.00786 AFIX 43 H27 2 0.415206 -0.106212 0.221636 11.00000 -1.20000 AFIX 0 C28 1 0.358119 -0.022587 0.178282 11.00000 0.01604 0.02112 = 0.01797 0.00212 0.00628 0.00586 AFIX 43 H28 2 0.286018 -0.064511 0.180868 11.00000 -1.20000 AFIX 0 C29 1 0.386918 0.063833 0.150650 11.00000 0.01735 0.02392 = 0.02233 0.00611 0.00518 0.01194 AFIX 43 H29 2 0.334316 0.080950 0.134260 11.00000 -1.20000 AFIX 0 C30 1 0.492627 0.125803 0.146760 11.00000 0.01912 0.01818 = 0.02061 0.00678 0.00576 0.01078 AFIX 43 H30 2 0.511979 0.185445 0.128324 11.00000 -1.20000 AFIX 0 C31 1 0.391936 0.370924 0.153913 11.00000 0.01616 0.01610 = 0.02037 0.00579 0.00775 0.01022 C32 1 0.340368 0.295832 0.190096 11.00000 0.02074 0.02206 = 0.02221 0.01010 0.00700 0.01007 AFIX 43 H32 2 0.382313 0.292932 0.232396 11.00000 -1.20000 AFIX 0 C33 1 0.227803 0.225163 0.164535 11.00000 0.02201 0.02493 = 0.03188 0.01450 0.00949 0.00654 AFIX 43 H33 2 0.193268 0.174814 0.189892 11.00000 -1.20000 AFIX 0 C34 1 0.165563 0.227535 0.102405 11.00000 0.01470 0.02522 = 0.03289 0.00703 0.00601 0.00831 AFIX 43 H34 2 0.088913 0.177754 0.084477 11.00000 -1.20000 AFIX 0 C35 1 0.215270 0.302474 0.066613 11.00000 0.02125 0.03088 = 0.02753 0.01036 0.00628 0.01839 AFIX 43 H35 2 0.172770 0.304913 0.024369 11.00000 -1.20000 AFIX 0 C36 1 0.327741 0.374406 0.092552 11.00000 0.01993 0.02455 = 0.02883 0.01478 0.01147 0.01559 AFIX 43 H36 2 0.361397 0.426589 0.068268 11.00000 -1.20000 AFIX 0 C37 1 0.583134 0.584051 0.180918 11.00000 0.01781 0.01490 = 0.01590 0.00528 0.00342 0.00921 C38 1 0.545295 0.643112 0.220289 11.00000 0.02372 0.02097 = 0.02135 0.00840 0.00924 0.01385 AFIX 43 H38 2 0.488981 0.608446 0.242232 11.00000 -1.20000 AFIX 0 C39 1 0.589380 0.752146 0.227599 11.00000 0.03103 0.02166 = 0.02356 0.00477 0.00653 0.01819 AFIX 43 H39 2 0.563754 0.791725 0.255096 11.00000 -1.20000 AFIX 0 C40 1 0.670563 0.803408 0.194956 11.00000 0.02633 0.01519 = 0.02413 0.00572 -0.00031 0.01035 AFIX 43 H40 2 0.700272 0.877799 0.199779 11.00000 -1.20000 AFIX 0 C41 1 0.708095 0.745485 0.155261 11.00000 0.02080 0.01916 = 0.02421 0.00999 0.00571 0.00815 AFIX 43 H41 2 0.763231 0.780175 0.132435 11.00000 -1.20000 AFIX 0 C42 1 0.665472 0.636854 0.148668 11.00000 0.01913 0.01782 = 0.01930 0.00626 0.00561 0.00996 AFIX 43 H42 2 0.692540 0.598157 0.122008 11.00000 -1.20000 AFIX 0 K1 7 0.269210 0.107845 0.533477 11.00000 0.01943 0.01895 = 0.01747 0.00479 0.00472 0.01034 O4 4 0.136272 0.024416 0.623484 11.00000 0.02944 0.04226 = 0.03389 0.01864 0.01563 0.01633 O5 4 0.152095 0.203833 0.583894 11.00000 0.02696 0.03478 = 0.02080 0.00083 0.00613 0.01851 O6 4 0.434879 0.063092 0.569450 11.00000 0.03217 0.04057 = 0.02310 0.00974 0.00267 0.02549 O7 4 0.489915 0.280546 0.593397 11.00000 0.02110 0.03029 = 0.03156 0.01169 0.01148 0.01029 O8 4 0.171422 -0.073243 0.399585 11.00000 0.02984 0.02249 = 0.02204 0.00119 0.00448 0.01587 O9 4 0.268671 0.136034 0.390656 11.00000 0.02932 0.02679 = 0.01807 0.00699 0.00561 0.01220 N6 3 0.207883 -0.109389 0.545693 11.00000 0.03630 0.02586 = 0.03021 0.00903 -0.00238 0.01695 N7 3 0.328896 0.321397 0.518577 11.00000 0.02803 0.01890 = 0.02785 0.00641 0.00688 0.01021 C43 1 0.166244 -0.121191 0.611699 11.00000 0.06760 0.03996 = 0.04198 0.02729 0.01037 0.02355 AFIX 23 H43A 2 0.228711 -0.077558 0.658633 11.00000 -1.20000 H43B 2 0.131111 -0.198193 0.609260 11.00000 -1.20000 AFIX 0 C44 1 0.085888 -0.086890 0.617165 11.00000 0.04894 0.04888 = 0.04618 0.02923 0.02274 0.01440 AFIX 23 H44A 2 0.021700 -0.131235 0.571334 11.00000 -1.20000 H44B 2 0.060743 -0.098362 0.662177 11.00000 -1.20000 AFIX 0 C45 1 0.066975 0.063815 0.636412 11.00000 0.03382 0.08028 = 0.04275 0.03387 0.02621 0.03472 AFIX 23 H45A 2 0.042438 0.047825 0.680855 11.00000 -1.20000 H45B 2 0.001738 0.026386 0.591564 11.00000 -1.20000 AFIX 0 C46 1 0.125177 0.182181 0.650427 11.00000 0.04033 0.06954 = 0.02372 0.01138 0.01519 0.04043 AFIX 23 H46A 2 0.078416 0.209751 0.663523 11.00000 -1.20000 H46B 2 0.192460 0.219632 0.693652 11.00000 -1.20000 AFIX 0 C47 1 0.203501 0.317572 0.595383 11.00000 0.03141 0.03067 = 0.04335 -0.00851 0.00668 0.01900 AFIX 23 H47A 2 0.266193 0.358811 0.642197 11.00000 -1.20000 H47B 2 0.151191 0.340454 0.601570 11.00000 -1.20000 AFIX 0 C48 1 0.241743 0.341118 0.528709 11.00000 0.03786 0.02310 = 0.05154 0.00729 0.00583 0.02049 AFIX 23 H48A 2 0.178791 0.295826 0.482145 11.00000 -1.20000 H48B 2 0.268279 0.418084 0.534220 11.00000 -1.20000 AFIX 0 C49 1 0.302172 -0.121348 0.555152 11.00000 0.04911 0.03165 = 0.04832 0.00431 -0.01234 0.02746 AFIX 23 H49A 2 0.310528 -0.143881 0.504520 11.00000 -1.20000 H49B 2 0.288323 -0.179694 0.577574 11.00000 -1.20000 AFIX 0 C50 1 0.406816 -0.018761 0.604933 11.00000 0.04436 0.03688 = 0.03488 0.01043 -0.00504 0.02692 AFIX 23 H50A 2 0.398090 0.006839 0.654821 11.00000 -1.20000 H50B 2 0.465966 -0.033459 0.613659 11.00000 -1.20000 AFIX 0 C51 1 0.540223 0.155057 0.610706 11.00000 0.02361 0.05545 = 0.03251 0.02023 0.00838 0.02356 AFIX 23 H51A 2 0.595605 0.135817 0.606802 11.00000 -1.20000 H51B 2 0.544893 0.178161 0.665046 11.00000 -1.20000 AFIX 0 C52 1 0.562876 0.246280 0.579973 11.00000 0.02342 0.05805 = 0.03821 0.02597 0.01485 0.02308 AFIX 23 H52A 2 0.639103 0.307505 0.605314 11.00000 -1.20000 H52B 2 0.552849 0.221855 0.524745 11.00000 -1.20000 AFIX 0 C53 1 0.521535 0.381200 0.580299 11.00000 0.02484 0.02669 = 0.03404 0.00966 0.00801 0.00333 AFIX 23 H53A 2 0.537833 0.378388 0.531092 11.00000 -1.20000 H53B 2 0.588350 0.440674 0.620945 11.00000 -1.20000 AFIX 0 C54 1 0.431268 0.403275 0.579192 11.00000 0.03161 0.01820 = 0.03285 0.00508 0.00841 0.00611 AFIX 23 H54A 2 0.416508 0.406753 0.628912 11.00000 -1.20000 H54B 2 0.456343 0.475218 0.572872 11.00000 -1.20000 AFIX 0 C55 1 0.121196 -0.190720 0.475226 11.00000 0.03629 0.01904 = 0.04168 0.00736 -0.00453 0.00955 AFIX 23 H55A 2 0.055203 -0.187404 0.474282 11.00000 -1.20000 H55B 2 0.102858 -0.263866 0.475971 11.00000 -1.20000 AFIX 0 C56 1 0.150351 -0.176307 0.403704 11.00000 0.03549 0.02024 = 0.03438 -0.00356 -0.00641 0.01580 AFIX 23 H56A 2 0.215812 -0.180231 0.403438 11.00000 -1.20000 H56B 2 0.089617 -0.235152 0.358945 11.00000 -1.20000 AFIX 0 C57 1 0.218179 -0.047554 0.340374 11.00000 0.03066 0.03820 = 0.02056 -0.00133 0.00601 0.02174 AFIX 23 H57A 2 0.179069 -0.112163 0.294020 11.00000 -1.20000 H57B 2 0.295531 -0.025661 0.355893 11.00000 -1.20000 AFIX 0 C58 1 0.210327 0.042993 0.324130 11.00000 0.02781 0.03584 = 0.01549 0.00376 0.00649 0.01486 AFIX 23 H58A 2 0.241306 0.060362 0.282182 11.00000 -1.20000 H58B 2 0.132939 0.020898 0.308258 11.00000 -1.20000 AFIX 0 C59 1 0.258850 0.222657 0.379192 11.00000 0.04418 0.03139 = 0.02688 0.01557 0.00711 0.01621 AFIX 23 H59A 2 0.184731 0.206895 0.377786 11.00000 -1.20000 H59B 2 0.270755 0.231284 0.330083 11.00000 -1.20000 AFIX 0 C60 1 0.342560 0.325686 0.443446 11.00000 0.04329 0.02448 = 0.03379 0.01685 0.00938 0.01158 AFIX 23 H60A 2 0.416108 0.340563 0.443729 11.00000 -1.20000 H60B 2 0.338152 0.386804 0.434044 11.00000 -1.20000 AFIX 0 CL1 6 0.499994 0.218239 0.359729 11.00000 0.04029 0.04024 = 0.03515 0.01792 0.01055 0.01754 CL2 6 0.728279 0.386139 0.433725 11.00000 0.04343 0.02340 = 0.06505 0.01147 0.00508 0.01567 C61 1 0.625585 0.304702 0.345909 11.00000 0.04317 0.04789 = 0.03828 0.02884 0.02623 0.03353 AFIX 23 H61A 2 0.646960 0.260465 0.314249 11.00000 -1.20000 H61B 2 0.617410 0.351791 0.318568 11.00000 -1.20000 AFIX 0 CL3 6 1.105391 0.366740 0.346207 11.00000 0.04935 0.06097 = 0.08795 0.02533 -0.01047 0.02771 PART 1 CL4A 6 1.028106 0.493030 0.421102 10.58000 0.09312 0.09282 = 0.03553 -0.01979 -0.00232 0.04075 PART 0 PART 2 CL4B 6 1.079522 0.548928 0.362264 10.42000 0.09232 0.05308 = 0.09658 0.02189 0.02354 0.04157 C62B 1 1.016392 0.421220 0.369235 10.35000 0.05976 AFIX 23 H62A 2 0.942265 0.374745 0.332690 10.35000 -1.20000 H62B 2 1.010656 0.423946 0.421229 10.35000 -1.20000 AFIX 0 PART 0 PART 1 C62 1 1.031312 0.429199 0.332008 10.65000 0.03659 AFIX 23 H62C 2 0.956125 0.374123 0.298928 10.65000 -1.20000 H62D 2 1.066299 0.483668 0.306747 10.65000 -1.20000 AFIX 0 HKLF 4 REM asb550 in P-1 REM R1 = 0.0365 for 13000 Fo > 4sig(Fo) and 0.0421 for all 14722 data REM 804 parameters refined using 0 restraints END WGHT 0.0430 3.1920 REM Highest difference peak 0.912, deepest hole -0.916, 1-sigma level 0.059 Q1 1 1.0799 0.5481 0.4156 11.00000 0.05 0.91 Q2 1 1.0679 0.3522 0.3802 11.00000 0.05 0.86 Q3 1 1.0750 0.4107 0.3482 11.00000 0.05 0.78 Q4 1 0.7354 0.4089 0.4771 11.00000 0.05 0.73 Q5 1 0.9842 0.5066 0.4253 11.00000 0.05 0.73 Q6 1 0.5443 0.2312 0.3376 11.00000 0.05 0.64 Q7 1 1.0081 0.4533 0.3410 11.00000 0.05 0.54 Q8 1 0.5603 0.4182 0.1424 11.00000 0.05 0.41 Q9 1 0.8960 0.5819 0.1283 11.00000 0.05 0.41 Q10 1 0.5619 0.5194 0.1804 11.00000 0.05 0.41 ; _shelx_res_checksum 16305 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.72439(2) 0.40069(2) 0.12998(2) 0.01153(6) Uani 1 1 d . . . . . P1 P 0.71070(3) 0.18853(3) 0.17135(2) 0.01407(9) Uani 1 1 d . . . . . P2 P 0.96259(3) 0.62429(3) 0.16246(2) 0.01509(9) Uani 1 1 d . . . . . P3 P 0.54021(3) 0.44634(3) 0.18001(2) 0.01355(9) Uani 1 1 d . . . . . O1 O 0.77782(10) 0.26113(10) 0.25116(7) 0.0189(3) Uani 1 1 d . . . . . O2 O 0.95949(10) 0.66742(10) 0.24049(7) 0.0219(3) Uani 1 1 d . . . . . O3 O 0.58495(10) 0.45052(10) 0.25853(7) 0.0182(2) Uani 1 1 d . . . . . N1 N 0.66104(11) 0.33743(11) 0.00401(8) 0.0135(3) Uani 1 1 d . . . . . N2 N 0.84672(11) 0.52805(11) 0.10325(8) 0.0154(3) Uani 1 1 d . . . . . N3 N 0.71320(11) 0.25015(11) 0.10984(8) 0.0147(3) Uani 1 1 d . . . . . N4 N 0.57465(11) 0.39172(11) 0.11482(8) 0.0146(3) Uani 1 1 d . . . . . N5 N 0.79015(13) 0.46781(13) 0.25130(8) 0.0170(3) Uani 1 1 d . . . . . H5A H 0.806(2) 0.426(2) 0.2686(16) 0.051(8) Uiso 1 1 d . . . . . H5B H 0.844(2) 0.529(2) 0.2630(14) 0.035(7) Uiso 1 1 d . . . . . H5C H 0.745(2) 0.4739(19) 0.2666(14) 0.029(6) Uiso 1 1 d . . . . . C1 C 0.71943(15) 0.42867(14) -0.02377(10) 0.0183(3) Uani 1 1 d . . . . . H1A H 0.6861 0.4730 -0.0199 0.022 Uiso 1 1 calc R U . . . H1B H 0.7129 0.4004 -0.0779 0.022 Uiso 1 1 calc R U . . . C2 C 0.83901(14) 0.49916(14) 0.02225(10) 0.0174(3) Uani 1 1 d . . . . . H2A H 0.8759 0.4591 0.0117 0.021 Uiso 1 1 calc R U . . . H2B H 0.8752 0.5658 0.0081 0.021 Uiso 1 1 calc R U . . . C3 C 0.68377(14) 0.25207(14) -0.02105(10) 0.0177(3) Uani 1 1 d . . . . . H3A H 0.7612 0.2857 -0.0197 0.021 Uiso 1 1 calc R U . . . H3B H 0.6383 0.2066 -0.0741 0.021 Uiso 1 1 calc R U . . . C4 C 0.65986(14) 0.18125(13) 0.02965(10) 0.0171(3) Uani 1 1 d . . . . . H4A H 0.5802 0.1359 0.0205 0.021 Uiso 1 1 calc R U . . . H4B H 0.6871 0.1323 0.0175 0.021 Uiso 1 1 calc R U . . . C5 C 0.54385(14) 0.29468(14) -0.01659(10) 0.0181(3) Uani 1 1 d . . . . . H5D H 0.5044 0.2210 -0.0124 0.022 Uiso 1 1 calc R U . . . H5E H 0.5177 0.2891 -0.0700 0.022 Uiso 1 1 calc R U . . . C6 C 0.51980(14) 0.36846(14) 0.03536(10) 0.0176(3) Uani 1 1 d . . . . . H6A H 0.5460 0.4371 0.0236 0.021 Uiso 1 1 calc R U . . . H6B H 0.4402 0.3326 0.0270 0.021 Uiso 1 1 calc R U . . . C7 C 1.02127(13) 0.73576(14) 0.12411(10) 0.0173(3) Uani 1 1 d . . . . . C8 C 1.01569(14) 0.82645(14) 0.15464(11) 0.0211(4) Uani 1 1 d . . . . . H8 H 0.9867 0.8302 0.1961 0.025 Uiso 1 1 calc R U . . . C9 C 1.05235(15) 0.91114(15) 0.12461(12) 0.0262(4) Uani 1 1 d . . . . . H9 H 1.0496 0.9731 0.1465 0.031 Uiso 1 1 calc R U . . . C10 C 1.09267(15) 0.90609(16) 0.06338(12) 0.0266(4) Uani 1 1 d . . . . . H10 H 1.1166 0.9639 0.0427 0.032 Uiso 1 1 calc R U . . . C11 C 1.09823(15) 0.81640(16) 0.03201(11) 0.0244(4) Uani 1 1 d . . . . . H11 H 1.1255 0.8124 -0.0103 0.029 Uiso 1 1 calc R U . . . C12 C 1.06369(14) 0.73232(15) 0.06284(11) 0.0208(4) Uani 1 1 d . . . . . H12 H 1.0690 0.6717 0.0419 0.025 Uiso 1 1 calc R U . . . C13 C 1.05730(14) 0.57789(14) 0.16950(10) 0.0172(3) Uani 1 1 d . . . . . C14 C 1.16948(15) 0.64980(15) 0.20260(11) 0.0237(4) Uani 1 1 d . . . . . H14 H 1.1992 0.7258 0.2168 0.028 Uiso 1 1 calc R U . . . C15 C 1.23804(16) 0.61143(17) 0.21491(11) 0.0265(4) Uani 1 1 d . . . . . H15 H 1.3142 0.6613 0.2376 0.032 Uiso 1 1 calc R U . . . C16 C 1.19599(16) 0.50085(17) 0.19424(11) 0.0259(4) Uani 1 1 d . . . . . H16 H 1.2430 0.4748 0.2032 0.031 Uiso 1 1 calc R U . . . C17 C 1.08501(17) 0.42833(16) 0.16051(12) 0.0273(4) Uani 1 1 d . . . . . H17 H 1.0560 0.3524 0.1458 0.033 Uiso 1 1 calc R U . . . C18 C 1.01612(15) 0.46650(15) 0.14816(11) 0.0221(4) Uani 1 1 d . . . . . H18 H 0.9401 0.4163 0.1249 0.026 Uiso 1 1 calc R U . . . C19 C 0.75539(14) 0.09562(14) 0.14069(10) 0.0163(3) Uani 1 1 d . . . . . C20 C 0.86130(15) 0.12689(15) 0.17778(11) 0.0205(4) Uani 1 1 d . . . . . H20 H 0.9045 0.1909 0.2207 0.025 Uiso 1 1 calc R U . . . C21 C 0.90386(15) 0.06480(16) 0.15212(12) 0.0242(4) Uani 1 1 d . . . . . H21 H 0.9759 0.0865 0.1778 0.029 Uiso 1 1 calc R U . . . C22 C 0.84163(15) -0.02860(15) 0.08916(11) 0.0228(4) Uani 1 1 d . . . . . H22 H 0.8714 -0.0701 0.0713 0.027 Uiso 1 1 calc R U . . . C23 C 0.73603(15) -0.06108(14) 0.05242(11) 0.0209(4) Uani 1 1 d . . . . . H23 H 0.6931 -0.1251 0.0095 0.025 Uiso 1 1 calc R U . . . C24 C 0.69290(14) 0.00001(14) 0.07838(11) 0.0189(3) Uani 1 1 d . . . . . H24 H 0.6200 -0.0234 0.0535 0.023 Uiso 1 1 calc R U . . . C25 C 0.57004(13) 0.10046(13) 0.16987(9) 0.0156(3) Uani 1 1 d . . . . . C26 C 0.53989(14) 0.01286(14) 0.19740(10) 0.0180(3) Uani 1 1 d . . . . . H26 H 0.5917 -0.0055 0.2130 0.022 Uiso 1 1 calc R U . . . C27 C 0.43457(15) -0.04760(14) 0.20206(10) 0.0196(4) Uani 1 1 d . . . . . H27 H 0.4152 -0.1062 0.2216 0.024 Uiso 1 1 calc R U . . . C28 C 0.35812(15) -0.02259(15) 0.17828(10) 0.0208(4) Uani 1 1 d . . . . . H28 H 0.2860 -0.0645 0.1809 0.025 Uiso 1 1 calc R U . . . C29 C 0.38692(15) 0.06383(15) 0.15065(11) 0.0211(4) Uani 1 1 d . . . . . H29 H 0.3343 0.0809 0.1343 0.025 Uiso 1 1 calc R U . . . C30 C 0.49263(14) 0.12580(14) 0.14676(10) 0.0188(3) Uani 1 1 d . . . . . H30 H 0.5120 0.1854 0.1283 0.023 Uiso 1 1 calc R U . . . C31 C 0.39194(14) 0.37092(14) 0.15391(10) 0.0165(3) Uani 1 1 d . . . . . C32 C 0.34037(15) 0.29583(15) 0.19010(11) 0.0217(4) Uani 1 1 d . . . . . H32 H 0.3823 0.2929 0.2324 0.026 Uiso 1 1 calc R U . . . C33 C 0.22780(16) 0.22516(16) 0.16454(12) 0.0279(4) Uani 1 1 d . . . . . H33 H 0.1933 0.1748 0.1899 0.033 Uiso 1 1 calc R U . . . C34 C 0.16556(15) 0.22754(16) 0.10241(12) 0.0259(4) Uani 1 1 d . . . . . H34 H 0.0889 0.1778 0.0845 0.031 Uiso 1 1 calc R U . . . C35 C 0.21527(15) 0.30247(16) 0.06661(11) 0.0244(4) Uani 1 1 d . . . . . H35 H 0.1728 0.3049 0.0244 0.029 Uiso 1 1 calc R U . . . C36 C 0.32774(15) 0.37441(15) 0.09255(11) 0.0210(4) Uani 1 1 d . . . . . H36 H 0.3614 0.4266 0.0683 0.025 Uiso 1 1 calc R U . . . C37 C 0.58313(14) 0.58405(13) 0.18092(10) 0.0161(3) Uani 1 1 d . . . . . C38 C 0.54529(15) 0.64311(15) 0.22029(10) 0.0205(4) Uani 1 1 d . . . . . H38 H 0.4890 0.6084 0.2422 0.025 Uiso 1 1 calc R U . . . C39 C 0.58938(16) 0.75215(15) 0.22760(11) 0.0242(4) Uani 1 1 d . . . . . H39 H 0.5638 0.7917 0.2551 0.029 Uiso 1 1 calc R U . . . C40 C 0.67056(16) 0.80341(15) 0.19496(11) 0.0234(4) Uani 1 1 d . . . . . H40 H 0.7003 0.8778 0.1998 0.028 Uiso 1 1 calc R U . . . C41 C 0.70810(15) 0.74549(15) 0.15526(11) 0.0221(4) Uani 1 1 d . . . . . H41 H 0.7632 0.7802 0.1324 0.027 Uiso 1 1 calc R U . . . C42 C 0.66547(14) 0.63685(14) 0.14867(10) 0.0187(3) Uani 1 1 d . . . . . H42 H 0.6925 0.5982 0.1220 0.022 Uiso 1 1 calc R U . . . K1 K 0.26921(3) 0.10785(3) 0.53348(2) 0.01886(8) Uani 1 1 d . . . . . O4 O 0.13627(12) 0.02442(13) 0.62348(9) 0.0345(3) Uani 1 1 d . . . . . O5 O 0.15210(11) 0.20383(12) 0.58389(8) 0.0281(3) Uani 1 1 d . . . . . O6 O 0.43488(12) 0.06309(12) 0.56945(8) 0.0299(3) Uani 1 1 d . . . . . O7 O 0.48992(11) 0.28055(12) 0.59340(8) 0.0284(3) Uani 1 1 d . . . . . O8 O 0.17142(11) -0.07324(11) 0.39958(8) 0.0254(3) Uani 1 1 d . . . . . O9 O 0.26867(11) 0.13603(11) 0.39066(7) 0.0262(3) Uani 1 1 d . . . . . N6 N 0.20788(15) -0.10939(14) 0.54569(10) 0.0322(4) Uani 1 1 d . . . . . N7 N 0.32890(14) 0.32140(13) 0.51858(10) 0.0264(4) Uani 1 1 d . . . . . C43 C 0.1662(3) -0.1212(2) 0.61170(15) 0.0505(7) Uani 1 1 d . . . . . H43A H 0.2287 -0.0776 0.6586 0.061 Uiso 1 1 calc R U . . . H43B H 0.1311 -0.1982 0.6093 0.061 Uiso 1 1 calc R U . . . C44 C 0.0859(2) -0.0869(2) 0.61716(16) 0.0498(7) Uani 1 1 d . . . . . H44A H 0.0217 -0.1312 0.5713 0.060 Uiso 1 1 calc R U . . . H44B H 0.0607 -0.0984 0.6622 0.060 Uiso 1 1 calc R U . . . C45 C 0.0670(2) 0.0638(2) 0.63641(15) 0.0458(6) Uani 1 1 d . . . . . H45A H 0.0424 0.0478 0.6809 0.055 Uiso 1 1 calc R U . . . H45B H 0.0017 0.0264 0.5916 0.055 Uiso 1 1 calc R U . . . C46 C 0.1252(2) 0.1822(2) 0.65043(12) 0.0393(6) Uani 1 1 d . . . . . H46A H 0.0784 0.2098 0.6635 0.047 Uiso 1 1 calc R U . . . H46B H 0.1925 0.2196 0.6937 0.047 Uiso 1 1 calc R U . . . C47 C 0.20350(19) 0.31757(18) 0.59538(14) 0.0382(5) Uani 1 1 d . . . . . H47A H 0.2662 0.3588 0.6422 0.046 Uiso 1 1 calc R U . . . H47B H 0.1512 0.3405 0.6016 0.046 Uiso 1 1 calc R U . . . C48 C 0.24174(19) 0.34112(18) 0.52871(15) 0.0374(5) Uani 1 1 d . . . . . H48A H 0.1788 0.2958 0.4821 0.045 Uiso 1 1 calc R U . . . H48B H 0.2683 0.4181 0.5342 0.045 Uiso 1 1 calc R U . . . C49 C 0.3022(2) -0.12135(19) 0.55515(15) 0.0454(6) Uani 1 1 d . . . . . H49A H 0.3105 -0.1439 0.5045 0.054 Uiso 1 1 calc R U . . . H49B H 0.2883 -0.1797 0.5776 0.054 Uiso 1 1 calc R U . . . C50 C 0.4068(2) -0.01876(19) 0.60493(14) 0.0387(5) Uani 1 1 d . . . . . H50A H 0.3981 0.0068 0.6548 0.046 Uiso 1 1 calc R U . . . H50B H 0.4660 -0.0335 0.6137 0.046 Uiso 1 1 calc R U . . . C51 C 0.54022(17) 0.1551(2) 0.61071(13) 0.0350(5) Uani 1 1 d . . . . . H51A H 0.5956 0.1358 0.6068 0.042 Uiso 1 1 calc R U . . . H51B H 0.5449 0.1782 0.6650 0.042 Uiso 1 1 calc R U . . . C52 C 0.56288(18) 0.2463(2) 0.57997(14) 0.0366(5) Uani 1 1 d . . . . . H52A H 0.6391 0.3075 0.6053 0.044 Uiso 1 1 calc R U . . . H52B H 0.5528 0.2219 0.5247 0.044 Uiso 1 1 calc R U . . . C53 C 0.52153(17) 0.38120(17) 0.58030(13) 0.0335(5) Uani 1 1 d . . . . . H53A H 0.5378 0.3784 0.5311 0.040 Uiso 1 1 calc R U . . . H53B H 0.5883 0.4407 0.6209 0.040 Uiso 1 1 calc R U . . . C54 C 0.43127(17) 0.40328(16) 0.57919(13) 0.0316(5) Uani 1 1 d . . . . . H54A H 0.4165 0.4068 0.6289 0.038 Uiso 1 1 calc R U . . . H54B H 0.4563 0.4752 0.5729 0.038 Uiso 1 1 calc R U . . . C55 C 0.12120(19) -0.19072(17) 0.47523(13) 0.0373(5) Uani 1 1 d . . . . . H55A H 0.0552 -0.1874 0.4743 0.045 Uiso 1 1 calc R U . . . H55B H 0.1029 -0.2639 0.4760 0.045 Uiso 1 1 calc R U . . . C56 C 0.15035(19) -0.17631(16) 0.40370(13) 0.0340(5) Uani 1 1 d . . . . . H56A H 0.2158 -0.1802 0.4034 0.041 Uiso 1 1 calc R U . . . H56B H 0.0896 -0.2352 0.3589 0.041 Uiso 1 1 calc R U . . . C57 C 0.21818(18) -0.04755(18) 0.34037(11) 0.0304(4) Uani 1 1 d . . . . . H57A H 0.1791 -0.1122 0.2940 0.036 Uiso 1 1 calc R U . . . H57B H 0.2955 -0.0257 0.3559 0.036 Uiso 1 1 calc R U . . . C58 C 0.21033(17) 0.04299(17) 0.32413(11) 0.0281(4) Uani 1 1 d . . . . . H58A H 0.2413 0.0604 0.2822 0.034 Uiso 1 1 calc R U . . . H58B H 0.1329 0.0209 0.3083 0.034 Uiso 1 1 calc R U . . . C59 C 0.2589(2) 0.22266(18) 0.37919(12) 0.0353(5) Uani 1 1 d . . . . . H59A H 0.1847 0.2069 0.3778 0.042 Uiso 1 1 calc R U . . . H59B H 0.2708 0.2313 0.3301 0.042 Uiso 1 1 calc R U . . . C60 C 0.3426(2) 0.32569(17) 0.44345(13) 0.0358(5) Uani 1 1 d . . . . . H60A H 0.4161 0.3406 0.4437 0.043 Uiso 1 1 calc R U . . . H60B H 0.3382 0.3868 0.4340 0.043 Uiso 1 1 calc R U . . . Cl1 Cl 0.49999(5) 0.21824(5) 0.35973(3) 0.03943(13) Uani 1 1 d . . . . . Cl2 Cl 0.72828(5) 0.38614(4) 0.43372(4) 0.04692(16) Uani 1 1 d . . . . . C61 C 0.62559(19) 0.3047(2) 0.34591(13) 0.0343(5) Uani 1 1 d . . . . . H61A H 0.6470 0.2605 0.3142 0.041 Uiso 1 1 calc R U . . . H61B H 0.6174 0.3518 0.3186 0.041 Uiso 1 1 calc R U . . . Cl3 Cl 1.10539(6) 0.36674(7) 0.34621(5) 0.0707(2) Uani 1 1 d . . . . . Cl4A Cl 1.02811(15) 0.49303(15) 0.42110(8) 0.0879(5) Uani 0.58 1 d . . P A 1 Cl4B Cl 1.0795(2) 0.54893(17) 0.36226(15) 0.0804(6) Uani 0.42 1 d . . P B 2 C62B C 1.0164(8) 0.4212(8) 0.3692(6) 0.060(2) Uiso 0.35 1 d . . P B 2 H62A H 0.9423 0.3747 0.3327 0.072 Uiso 0.35 1 calc R U P B 2 H62B H 1.0107 0.4239 0.4212 0.072 Uiso 0.35 1 calc R U P B 2 C62 C 1.0313(3) 0.4292(3) 0.3320(2) 0.0366(8) Uiso 0.65 1 d . . P A 1 H62C H 0.9561 0.3741 0.2989 0.044 Uiso 0.65 1 calc R U P A 1 H62D H 1.0663 0.4837 0.3067 0.044 Uiso 0.65 1 calc R U P A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01116(11) 0.01105(11) 0.01167(11) 0.00317(9) 0.00317(9) 0.00567(9) P1 0.01275(19) 0.01253(19) 0.0170(2) 0.00481(16) 0.00287(16) 0.00720(16) P2 0.0133(2) 0.01274(19) 0.0161(2) 0.00217(16) 0.00535(16) 0.00531(16) P3 0.0136(2) 0.01374(19) 0.0161(2) 0.00624(16) 0.00574(16) 0.00843(16) O1 0.0182(6) 0.0189(6) 0.0181(6) 0.0049(5) 0.0014(5) 0.0103(5) O2 0.0192(6) 0.0198(6) 0.0186(6) -0.0003(5) 0.0058(5) 0.0069(5) O3 0.0205(6) 0.0209(6) 0.0173(6) 0.0079(5) 0.0071(5) 0.0130(5) N1 0.0140(7) 0.0119(6) 0.0133(7) 0.0031(5) 0.0036(5) 0.0065(5) N2 0.0136(7) 0.0144(7) 0.0143(7) 0.0033(5) 0.0048(5) 0.0051(6) N3 0.0156(7) 0.0124(6) 0.0150(7) 0.0035(5) 0.0033(5) 0.0073(6) N4 0.0138(7) 0.0163(7) 0.0147(7) 0.0048(5) 0.0034(5) 0.0090(6) N5 0.0150(7) 0.0177(8) 0.0139(7) 0.0042(6) 0.0039(6) 0.0058(7) C1 0.0230(9) 0.0176(8) 0.0146(8) 0.0074(7) 0.0061(7) 0.0101(7) C2 0.0189(8) 0.0155(8) 0.0151(8) 0.0045(6) 0.0068(7) 0.0068(7) C3 0.0197(8) 0.0177(8) 0.0160(8) 0.0022(7) 0.0059(7) 0.0113(7) C4 0.0184(8) 0.0130(8) 0.0181(8) 0.0026(6) 0.0038(7) 0.0085(7) C5 0.0145(8) 0.0193(8) 0.0162(8) 0.0021(7) 0.0007(6) 0.0085(7) C6 0.0161(8) 0.0209(8) 0.0161(8) 0.0046(7) 0.0019(6) 0.0114(7) C7 0.0117(8) 0.0140(8) 0.0223(9) 0.0038(7) 0.0038(7) 0.0051(6) C8 0.0157(8) 0.0174(8) 0.0249(9) 0.0016(7) 0.0023(7) 0.0082(7) C9 0.0187(9) 0.0158(8) 0.0387(11) 0.0048(8) -0.0014(8) 0.0097(7) C10 0.0150(9) 0.0218(9) 0.0372(11) 0.0152(8) 0.0007(8) 0.0056(7) C11 0.0145(8) 0.0272(10) 0.0281(10) 0.0120(8) 0.0068(7) 0.0074(7) C12 0.0148(8) 0.0182(8) 0.0280(10) 0.0061(7) 0.0080(7) 0.0078(7) C13 0.0176(8) 0.0197(8) 0.0149(8) 0.0056(7) 0.0062(7) 0.0099(7) C14 0.0197(9) 0.0203(9) 0.0245(9) 0.0018(7) 0.0055(7) 0.0083(7) C15 0.0168(9) 0.0325(10) 0.0241(10) 0.0035(8) 0.0034(7) 0.0117(8) C16 0.0280(10) 0.0362(11) 0.0235(9) 0.0113(8) 0.0097(8) 0.0230(9) C17 0.0283(10) 0.0238(9) 0.0339(11) 0.0112(8) 0.0090(8) 0.0162(8) C18 0.0186(9) 0.0187(9) 0.0257(9) 0.0065(7) 0.0052(7) 0.0083(7) C19 0.0166(8) 0.0151(8) 0.0217(9) 0.0093(7) 0.0076(7) 0.0099(7) C20 0.0179(8) 0.0199(9) 0.0241(9) 0.0079(7) 0.0051(7) 0.0104(7) C21 0.0165(9) 0.0273(10) 0.0328(10) 0.0116(8) 0.0065(8) 0.0140(8) C22 0.0243(9) 0.0237(9) 0.0333(10) 0.0150(8) 0.0162(8) 0.0177(8) C23 0.0226(9) 0.0152(8) 0.0273(10) 0.0086(7) 0.0102(8) 0.0103(7) C24 0.0161(8) 0.0156(8) 0.0267(9) 0.0091(7) 0.0065(7) 0.0086(7) C25 0.0144(8) 0.0146(8) 0.0150(8) 0.0030(6) 0.0039(6) 0.0065(6) C26 0.0196(8) 0.0191(8) 0.0159(8) 0.0053(7) 0.0040(7) 0.0113(7) C27 0.0227(9) 0.0171(8) 0.0156(8) 0.0056(7) 0.0064(7) 0.0079(7) C28 0.0160(8) 0.0211(9) 0.0180(9) 0.0021(7) 0.0063(7) 0.0059(7) C29 0.0174(8) 0.0239(9) 0.0223(9) 0.0061(7) 0.0052(7) 0.0119(7) C30 0.0191(8) 0.0182(8) 0.0206(9) 0.0068(7) 0.0058(7) 0.0108(7) C31 0.0162(8) 0.0161(8) 0.0204(8) 0.0058(7) 0.0078(7) 0.0102(7) C32 0.0207(9) 0.0221(9) 0.0222(9) 0.0101(7) 0.0070(7) 0.0101(7) C33 0.0220(9) 0.0249(10) 0.0319(11) 0.0145(8) 0.0095(8) 0.0065(8) C34 0.0147(8) 0.0252(9) 0.0329(11) 0.0070(8) 0.0060(8) 0.0083(8) C35 0.0212(9) 0.0309(10) 0.0275(10) 0.0104(8) 0.0063(8) 0.0184(8) C36 0.0199(9) 0.0245(9) 0.0288(10) 0.0148(8) 0.0115(7) 0.0156(8) C37 0.0178(8) 0.0149(8) 0.0159(8) 0.0053(6) 0.0034(6) 0.0092(7) C38 0.0237(9) 0.0210(9) 0.0214(9) 0.0084(7) 0.0092(7) 0.0139(8) C39 0.0310(10) 0.0217(9) 0.0236(9) 0.0048(7) 0.0065(8) 0.0182(8) C40 0.0263(9) 0.0152(8) 0.0241(9) 0.0057(7) -0.0003(8) 0.0104(7) C41 0.0208(9) 0.0192(9) 0.0242(9) 0.0100(7) 0.0057(7) 0.0082(7) C42 0.0191(8) 0.0178(8) 0.0193(8) 0.0063(7) 0.0056(7) 0.0100(7) K1 0.01943(18) 0.01895(18) 0.01747(18) 0.00479(14) 0.00472(14) 0.01034(15) O4 0.0294(8) 0.0423(9) 0.0339(8) 0.0186(7) 0.0156(7) 0.0163(7) O5 0.0270(7) 0.0348(8) 0.0208(7) 0.0008(6) 0.0061(6) 0.0185(6) O6 0.0322(8) 0.0406(8) 0.0231(7) 0.0097(6) 0.0027(6) 0.0255(7) O7 0.0211(7) 0.0303(7) 0.0316(8) 0.0117(6) 0.0115(6) 0.0103(6) O8 0.0298(7) 0.0225(7) 0.0220(7) 0.0012(5) 0.0045(6) 0.0159(6) O9 0.0293(7) 0.0268(7) 0.0181(6) 0.0070(5) 0.0056(6) 0.0122(6) N6 0.0363(10) 0.0259(9) 0.0302(9) 0.0090(7) -0.0024(8) 0.0169(8) N7 0.0280(9) 0.0189(8) 0.0278(9) 0.0064(7) 0.0069(7) 0.0102(7) C43 0.0676(18) 0.0400(14) 0.0420(14) 0.0273(12) 0.0104(13) 0.0235(13) C44 0.0489(15) 0.0489(15) 0.0462(15) 0.0292(13) 0.0227(12) 0.0144(12) C45 0.0338(12) 0.0803(19) 0.0428(14) 0.0339(14) 0.0262(11) 0.0347(13) C46 0.0403(13) 0.0695(17) 0.0237(11) 0.0114(11) 0.0152(9) 0.0404(13) C47 0.0314(11) 0.0307(11) 0.0434(13) -0.0085(10) 0.0067(10) 0.0190(10) C48 0.0379(12) 0.0231(10) 0.0515(14) 0.0073(10) 0.0058(11) 0.0205(10) C49 0.0491(14) 0.0317(12) 0.0483(14) 0.0043(11) -0.0123(12) 0.0275(11) C50 0.0444(13) 0.0369(12) 0.0349(12) 0.0104(10) -0.0050(10) 0.0269(11) C51 0.0236(10) 0.0555(14) 0.0325(11) 0.0202(11) 0.0084(9) 0.0236(10) C52 0.0234(10) 0.0580(15) 0.0382(12) 0.0260(11) 0.0149(9) 0.0231(11) C53 0.0248(10) 0.0267(10) 0.0340(11) 0.0097(9) 0.0080(9) 0.0033(8) C54 0.0316(11) 0.0182(9) 0.0328(11) 0.0051(8) 0.0084(9) 0.0061(8) C55 0.0363(12) 0.0190(10) 0.0417(13) 0.0074(9) -0.0045(10) 0.0096(9) C56 0.0355(12) 0.0202(10) 0.0344(12) -0.0036(8) -0.0064(9) 0.0158(9) C57 0.0307(11) 0.0382(11) 0.0206(10) -0.0013(8) 0.0060(8) 0.0217(9) C58 0.0278(10) 0.0358(11) 0.0155(9) 0.0038(8) 0.0065(8) 0.0149(9) C59 0.0442(13) 0.0314(11) 0.0269(11) 0.0156(9) 0.0071(9) 0.0162(10) C60 0.0433(13) 0.0245(10) 0.0338(12) 0.0168(9) 0.0094(10) 0.0116(10) Cl1 0.0403(3) 0.0402(3) 0.0352(3) 0.0179(2) 0.0106(2) 0.0175(3) Cl2 0.0434(3) 0.0234(3) 0.0651(4) 0.0115(3) 0.0051(3) 0.0157(2) C61 0.0432(13) 0.0479(13) 0.0383(12) 0.0288(11) 0.0262(10) 0.0335(11) Cl3 0.0493(4) 0.0610(5) 0.0879(6) 0.0253(4) -0.0105(4) 0.0277(4) Cl4A 0.0931(12) 0.0928(12) 0.0355(7) -0.0198(7) -0.0023(7) 0.0408(10) Cl4B 0.0923(16) 0.0531(11) 0.0966(17) 0.0219(11) 0.0235(13) 0.0416(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Fe1 N3 115.17(5) . . ? N4 Fe1 N2 115.67(6) . . ? N3 Fe1 N2 120.30(6) . . ? N4 Fe1 N5 100.77(6) . . ? N3 Fe1 N5 101.31(6) . . ? N2 Fe1 N5 97.95(6) . . ? N4 Fe1 N1 79.92(5) . . ? N3 Fe1 N1 80.26(5) . . ? N2 Fe1 N1 79.83(5) . . ? N5 Fe1 N1 177.74(6) . . ? O1 P1 N3 115.22(7) . . ? O1 P1 C19 109.36(8) . . ? N3 P1 C19 108.56(8) . . ? O1 P1 C25 109.07(8) . . ? N3 P1 C25 109.61(8) . . ? C19 P1 C25 104.48(8) . . ? O2 P2 N2 115.19(7) . . ? O2 P2 C7 108.81(8) . . ? N2 P2 C7 108.92(8) . . ? O2 P2 C13 108.80(8) . . ? N2 P2 C13 109.39(8) . . ? C7 P2 C13 105.28(8) . . ? O3 P3 N4 115.01(7) . . ? O3 P3 C31 109.38(8) . . ? N4 P3 C31 107.97(8) . . ? O3 P3 C37 108.64(7) . . ? N4 P3 C37 109.36(8) . . ? C31 P3 C37 106.11(8) . . ? C5 N1 C3 111.90(13) . . ? C5 N1 C1 111.63(13) . . ? C3 N1 C1 111.71(13) . . ? C5 N1 Fe1 107.45(10) . . ? C3 N1 Fe1 106.52(10) . . ? C1 N1 Fe1 107.29(10) . . ? C2 N2 P2 117.93(11) . . ? C2 N2 Fe1 112.70(10) . . ? P2 N2 Fe1 124.90(8) . . ? C4 N3 P1 116.41(11) . . ? C4 N3 Fe1 112.82(10) . . ? P1 N3 Fe1 125.90(8) . . ? C6 N4 P3 117.91(11) . . ? C6 N4 Fe1 113.18(10) . . ? P3 N4 Fe1 125.19(8) . . ? N1 C1 C2 110.70(14) . . ? N2 C2 C1 108.64(14) . . ? N1 C3 C4 110.91(14) . . ? N3 C4 C3 109.69(13) . . ? N1 C5 C6 110.62(14) . . ? N4 C6 C5 109.45(14) . . ? C12 C7 C8 118.49(17) . . ? C12 C7 P2 123.94(13) . . ? C8 C7 P2 117.39(14) . . ? C9 C8 C7 120.33(18) . . ? C10 C9 C8 120.63(18) . . ? C9 C10 C11 119.85(18) . . ? C10 C11 C12 119.76(18) . . ? C11 C12 C7 120.91(17) . . ? C14 C13 C18 118.38(17) . . ? C14 C13 P2 122.10(14) . . ? C18 C13 P2 119.20(13) . . ? C15 C14 C13 120.71(18) . . ? C16 C15 C14 120.30(18) . . ? C15 C16 C17 119.75(18) . . ? C16 C17 C18 120.08(18) . . ? C17 C18 C13 120.77(17) . . ? C20 C19 C24 118.59(16) . . ? C20 C19 P1 117.65(13) . . ? C24 C19 P1 123.54(13) . . ? C21 C20 C19 120.35(17) . . ? C22 C21 C20 120.36(17) . . ? C23 C22 C21 119.80(17) . . ? C22 C23 C24 119.99(17) . . ? C23 C24 C19 120.89(16) . . ? C30 C25 C26 118.87(16) . . ? C30 C25 P1 119.62(13) . . ? C26 C25 P1 121.30(13) . . ? C27 C26 C25 120.53(16) . . ? C28 C27 C26 120.18(17) . . ? C27 C28 C29 119.83(17) . . ? C28 C29 C30 120.41(17) . . ? C29 C30 C25 120.18(16) . . ? C32 C31 C36 118.50(16) . . ? C32 C31 P3 118.20(13) . . ? C36 C31 P3 122.72(13) . . ? C33 C32 C31 120.28(17) . . ? C34 C33 C32 120.58(18) . . ? C35 C34 C33 119.82(18) . . ? C34 C35 C36 119.87(18) . . ? C35 C36 C31 120.91(17) . . ? C42 C37 C38 118.52(16) . . ? C42 C37 P3 119.06(13) . . ? C38 C37 P3 122.02(13) . . ? C39 C38 C37 120.57(17) . . ? C40 C39 C38 120.34(17) . . ? C41 C40 C39 119.61(17) . . ? C40 C41 C42 120.34(17) . . ? C41 C42 C37 120.60(17) . . ? O4 K1 O9 143.91(5) . . ? O4 K1 O7 123.52(5) . . ? O9 K1 O7 89.60(4) . . ? O4 K1 O8 101.80(5) . . ? O9 K1 O8 59.22(4) . . ? O7 K1 O8 128.11(4) . . ? O4 K1 O6 104.38(5) . . ? O9 K1 O6 104.76(4) . . ? O7 K1 O6 60.21(4) . . ? O8 K1 O6 87.01(4) . . ? O4 K1 O5 60.05(5) . . ? O9 K1 O5 101.46(4) . . ? O7 K1 O5 103.86(4) . . ? O8 K1 O5 121.22(4) . . ? O6 K1 O5 148.85(4) . . ? O4 K1 N7 120.05(5) . . ? O9 K1 N7 60.52(4) . . ? O7 K1 N7 61.11(5) . . ? O8 K1 N7 118.51(5) . . ? O6 K1 N7 119.21(5) . . ? O5 K1 N7 61.41(5) . . ? O4 K1 N6 60.59(5) . . ? O9 K1 N6 118.52(5) . . ? O7 K1 N6 119.29(5) . . ? O8 K1 N6 60.53(5) . . ? O6 K1 N6 60.93(5) . . ? O5 K1 N6 119.03(5) . . ? N7 K1 N6 179.04(5) . . ? C44 O4 C45 111.54(19) . . ? C44 O4 K1 120.45(14) . . ? C45 O4 K1 117.11(13) . . ? C46 O5 C47 109.81(17) . . ? C46 O5 K1 111.58(12) . . ? C47 O5 K1 115.37(12) . . ? C51 O6 C50 110.45(16) . . ? C51 O6 K1 115.42(12) . . ? C50 O6 K1 113.42(13) . . ? C52 O7 C53 111.66(16) . . ? C52 O7 K1 112.42(13) . . ? C53 O7 K1 119.42(12) . . ? C57 O8 C56 111.39(16) . . ? C57 O8 K1 112.69(11) . . ? C56 O8 K1 120.43(11) . . ? C59 O9 C58 111.42(15) . . ? C59 O9 K1 117.41(12) . . ? C58 O9 K1 119.16(11) . . ? C49 N6 C55 110.82(18) . . ? C49 N6 C43 109.60(19) . . ? C55 N6 C43 110.0(2) . . ? C49 N6 K1 110.77(14) . . ? C55 N6 K1 106.84(12) . . ? C43 N6 K1 108.76(14) . . ? C60 N7 C48 108.86(18) . . ? C60 N7 C54 110.69(17) . . ? C48 N7 C54 110.01(17) . . ? C60 N7 K1 111.34(12) . . ? C48 N7 K1 108.78(12) . . ? C54 N7 K1 107.13(12) . . ? N6 C43 C44 114.5(2) . . ? O4 C44 C43 109.3(2) . . ? O4 C45 C46 110.48(19) . . ? O5 C46 C45 109.26(19) . . ? O5 C47 C48 109.48(17) . . ? N7 C48 C47 114.78(19) . . ? N6 C49 C50 113.18(19) . . ? O6 C50 C49 109.94(18) . . ? O6 C51 C52 110.24(17) . . ? O7 C52 C51 108.84(17) . . ? O7 C53 C54 110.03(16) . . ? N7 C54 C53 114.07(17) . . ? N6 C55 C56 114.28(19) . . ? O8 C56 C55 109.52(17) . . ? O8 C57 C58 109.28(16) . . ? O9 C58 C57 109.33(16) . . ? O9 C59 C60 108.89(17) . . ? N7 C60 C59 113.65(17) . . ? Cl2 C61 Cl1 110.80(12) . . ? Cl4B C62B Cl3 105.5(5) . . ? Cl3 C62 Cl4A 109.0(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 2.1044(14) . ? Fe1 N3 2.1099(14) . ? Fe1 N2 2.1116(14) . ? Fe1 N5 2.1428(15) . ? Fe1 N1 2.2196(14) . ? P1 O1 1.4963(13) . ? P1 N3 1.6129(15) . ? P1 C19 1.8242(17) . ? P1 C25 1.8264(17) . ? P2 O2 1.4937(13) . ? P2 N2 1.6084(14) . ? P2 C7 1.8226(18) . ? P2 C13 1.8235(18) . ? P3 O3 1.4976(13) . ? P3 N4 1.6111(14) . ? P3 C31 1.8216(17) . ? P3 C37 1.8239(17) . ? N1 C5 1.465(2) . ? N1 C3 1.467(2) . ? N1 C1 1.470(2) . ? N2 C2 1.467(2) . ? N3 C4 1.471(2) . ? N4 C6 1.466(2) . ? C1 C2 1.519(2) . ? C3 C4 1.519(2) . ? C5 C6 1.523(2) . ? C7 C12 1.397(3) . ? C7 C8 1.398(2) . ? C8 C9 1.389(3) . ? C9 C10 1.380(3) . ? C10 C11 1.388(3) . ? C11 C12 1.392(3) . ? C13 C14 1.396(3) . ? C13 C18 1.397(2) . ? C14 C15 1.387(3) . ? C15 C16 1.385(3) . ? C16 C17 1.386(3) . ? C17 C18 1.389(3) . ? C19 C20 1.396(2) . ? C19 C24 1.399(2) . ? C20 C21 1.392(3) . ? C21 C22 1.389(3) . ? C22 C23 1.385(3) . ? C23 C24 1.389(2) . ? C25 C30 1.395(2) . ? C25 C26 1.398(2) . ? C26 C27 1.392(2) . ? C27 C28 1.382(3) . ? C28 C29 1.386(3) . ? C29 C30 1.394(2) . ? C31 C32 1.394(2) . ? C31 C36 1.399(3) . ? C32 C33 1.391(3) . ? C33 C34 1.386(3) . ? C34 C35 1.381(3) . ? C35 C36 1.392(3) . ? C37 C42 1.398(2) . ? C37 C38 1.398(2) . ? C38 C39 1.391(3) . ? C39 C40 1.387(3) . ? C40 C41 1.386(3) . ? C41 C42 1.390(2) . ? K1 O4 2.7892(15) . ? K1 O9 2.8062(14) . ? K1 O7 2.8287(14) . ? K1 O8 2.8299(13) . ? K1 O6 2.8345(14) . ? K1 O5 2.8619(14) . ? K1 N7 2.9473(17) . ? K1 N6 2.9765(18) . ? O4 C44 1.418(3) . ? O4 C45 1.423(3) . ? O5 C46 1.424(3) . ? O5 C47 1.429(3) . ? O6 C51 1.418(3) . ? O6 C50 1.427(3) . ? O7 C52 1.422(3) . ? O7 C53 1.426(3) . ? O8 C57 1.422(3) . ? O8 C56 1.431(2) . ? O9 C59 1.417(3) . ? O9 C58 1.423(2) . ? N6 C49 1.466(3) . ? N6 C55 1.473(3) . ? N6 C43 1.474(3) . ? N7 C60 1.470(3) . ? N7 C48 1.473(3) . ? N7 C54 1.473(3) . ? C43 C44 1.501(4) . ? C45 C46 1.478(4) . ? C47 C48 1.492(4) . ? C49 C50 1.505(3) . ? C51 C52 1.495(3) . ? C53 C54 1.507(3) . ? C55 C56 1.501(3) . ? C57 C58 1.492(3) . ? C59 C60 1.509(3) . ? Cl1 C61 1.766(2) . ? Cl2 C61 1.764(3) . ? Cl3 C62 1.760(4) . ? Cl3 C62B 1.896(9) . ? Cl4A C62 1.768(4) . ? Cl4B C62B 1.710(10) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5A O1 0.86(3) 2.23(3) 2.988(2) 148(3) . N5 H5B O2 0.82(3) 2.12(3) 2.884(2) 155(2) . N5 H5C O3 0.80(3) 2.17(3) 2.922(2) 156(2) .